目的 建立頭風(fēng)痛丸中氧化前胡素、歐前胡素、異歐前胡素、洋川芎內(nèi)酯H、洋川芎內(nèi)酯I、洋川芎內(nèi)酯A、瑟丹酸內(nèi)酯、藁本內(nèi)酯的HPLC法測定方法及其化學(xué)計(jì)量學(xué)綜合質(zhì)量評價(jià)方法。方法 使用Waters Symmetryshield C₁₈柱（250 mm×4.6 mm，5 μm），以甲醇-0.1%冰醋酸溶液為流動(dòng)相，梯度洗脫，檢測波長分別為310 nm（0~22 min檢測氧化前胡素、歐前胡素和異歐前胡素）、280 nm（22~60 min檢測川洋川芎內(nèi)酯H、洋川芎內(nèi)酯I、洋川芎內(nèi)酯A、瑟丹酸內(nèi)酯、藁本內(nèi)酯），柱溫30℃，體積流量1.0 mL/min，進(jìn)樣量10 μL。采用統(tǒng)計(jì)軟件對頭風(fēng)痛丸中8種成分的含量數(shù)據(jù)進(jìn)行主成分分析與聚類分析。結(jié)果 8種成分的線性范圍分別為14.27~356.75、10.85~271.25、4.09~102.25、0.58~14.50、0.96~24.00、2.54~63.50、1.22~30.50、4.89~122.25 μg/mL（r ≥ 0.999 2）；平均加樣回收率分別為100.05%、99.50%、99.38%、97.32%、96.98%、97.78%、96.93%、98.91%，RSD值分別為0.66%、0.59%、1.13%、0.99%、1.22%、1.07%、1.41%和0.78%（n=9）。15批樣品提取出3個(gè)主成分，聚類分析分成2類。結(jié)論 以氧化前胡素、歐前胡素、異歐前胡素、洋川芎內(nèi)酯H、洋川芎內(nèi)酯I、洋川芎內(nèi)酯A、瑟丹酸內(nèi)酯、藁本內(nèi)酯同步測定的HPLC法可用于頭風(fēng)痛丸多指標(biāo)質(zhì)量評價(jià)。

Objective To establish a method for the determination of oxypeucedanin, imperatorin, isoimperatorin, senkyunolide H, senkyunolide I, senkyunolide A, sedanolide, and ligustilide in Toufengtong Pills by HPLC and its chemometrics quality evaluation. Methods The separation and detection was performed on a Waters Symmetryshield C₁₈ (250 mm×4.6 mm, 5 μm) with linear gradient elution of methanol-0.1% aqueous acetic acid. The detection wavelengths were set at 310 nm (0-22 min for oxypeucedanin, imperatorin, and isoimperatorin) and 280 nm (22-60 min for senkyunolide H, senkyunolide I, senkyunolide A, sedanolide, and ligustilide). The column temperature was 30℃, the flow rate was set at 1.0 mL/min, and the injection volume was 10 μL. The principal component analysis and cluster analysis were conducted for the content results of eight constituents in Toufengtong Pills by statistical software. Results The linear ranges of eight components were 14.27-356.75, 10.85-271.25, 4.09-102.25, 0.58-14.50, 0.96-24.00, 2.54-63.50, 1.22-30.50, 4.89-122.25 μg/mL(r ≥ 0.999 2), whose average recoveries were 100.05%, 99.50%, 99.38%, 97.32%, 96.98%, 97.78%, 96.93%, and 98.91% with the RSD values of 0.66%, 0.59%, 1.13%, 0.99%, 1.22%, 1.07%, 1.41%, and 0.78% (n=9), respectively. Three main components belonged to the samples of the 15 batches of samples, and the samples of 15 batches of Toufengtong Pills could be divided into 2 categories. Conclusion Simultaneous determination of oxypeucedanin, imperatorin, isoimperatorin, senkyunolide H, senkyunolide I, senkyunolide A, sedanolide, and ligustilide by HPLC can be used to evaluate the quality of Toufengtong Pills.

R286.02

河南省重大科技專項(xiàng)（創(chuàng)新示范專項(xiàng)）項(xiàng)目（191110311100）